CN102795872B - 在致密化之前多孔预成形体的刚性化 - Google Patents
在致密化之前多孔预成形体的刚性化 Download PDFInfo
- Publication number
- CN102795872B CN102795872B CN201210165477.6A CN201210165477A CN102795872B CN 102795872 B CN102795872 B CN 102795872B CN 201210165477 A CN201210165477 A CN 201210165477A CN 102795872 B CN102795872 B CN 102795872B
- Authority
- CN
- China
- Prior art keywords
- preform
- carbon
- precursor
- densification
- matrix
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000280 densification Methods 0.000 title claims abstract description 87
- 239000002243 precursor Substances 0.000 claims abstract description 117
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 87
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000003763 carbonization Methods 0.000 claims abstract description 42
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 230000010412 perfusion Effects 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 150000001721 carbon Chemical class 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims description 90
- 239000003153 chemical reaction reagent Substances 0.000 claims description 58
- 238000000034 method Methods 0.000 claims description 53
- 229920005989 resin Polymers 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 24
- 238000000197 pyrolysis Methods 0.000 claims description 18
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 12
- 238000003892 spreading Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 5
- 238000001721 transfer moulding Methods 0.000 claims description 4
- 239000000835 fiber Substances 0.000 description 24
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 description 21
- 230000008595 infiltration Effects 0.000 description 20
- 238000001764 infiltration Methods 0.000 description 20
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000011302 mesophase pitch Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000010008 shearing Methods 0.000 description 5
- 230000006641 stabilisation Effects 0.000 description 5
- 239000010426 asphalt Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000001467 acupuncture Methods 0.000 description 3
- 239000011294 coal tar pitch Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012705 liquid precursor Substances 0.000 description 3
- 210000003141 lower extremity Anatomy 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- -1 AR mesophase pitch Chemical compound 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- FNYLWPVRPXGIIP-UHFFFAOYSA-N Triamterene Chemical compound NC1=NC2=NC(N)=NC(N)=C2N=C1C1=CC=CC=C1 FNYLWPVRPXGIIP-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000011026 diafiltration Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
- F16D69/02—Composition of linings ; Methods of manufacturing
- F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C45/14778—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles the article consisting of a material with particular properties, e.g. porous, brittle
- B29C45/14786—Fibrous material or fibre containing material, e.g. fibre mats or fibre reinforced material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
- Braking Arrangements (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/117711 | 2011-05-27 | ||
| US13/117,711 US9127732B2 (en) | 2011-05-27 | 2011-05-27 | Rigidization of porous preform prior to densification |
| US13/117,711 | 2011-05-27 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102795872A CN102795872A (zh) | 2012-11-28 |
| CN102795872B true CN102795872B (zh) | 2016-09-21 |
Family
ID=46085456
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210165477.6A Expired - Fee Related CN102795872B (zh) | 2011-05-27 | 2012-05-25 | 在致密化之前多孔预成形体的刚性化 |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US9127732B2 (fr) |
| EP (1) | EP2527129A1 (fr) |
| CN (1) | CN102795872B (fr) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9127732B2 (en) | 2011-05-27 | 2015-09-08 | Honeywell International Inc. | Rigidization of porous preform prior to densification |
| US20140377462A1 (en) | 2012-06-21 | 2014-12-25 | Robert Davis | Suspended Thin Films on Low-Stress Carbon Nanotube Support Structures |
| US20150128828A1 (en) * | 2012-07-16 | 2015-05-14 | Honeywell International Inc. | Infiltration of densified carbon-carbon composite material with low viscosity resin |
| US9550701B2 (en) * | 2013-07-25 | 2017-01-24 | Honeywell International Inc. | Carbon-carbon composites including isotropic carbon encapsulating layer and methods of forming the same |
| KR20160140604A (ko) * | 2014-03-27 | 2016-12-07 | 블루 큐브 아이피 엘엘씨 | 탄소-탄소 복합체의 제조 방법 |
| US20180328429A1 (en) * | 2017-05-10 | 2018-11-15 | Honeywell International Inc. | Carbon-carbon composites including encapsulated isotropic carbon |
| IT201700089398A1 (it) * | 2017-08-03 | 2019-02-03 | Freni Brembo Spa | Preforma per la realizzazione di un componente di impianto frenante, costituita in un materiale composito ceramico fibro-rinforzato ottenuto per formatura e pirolisi di un pre-preg |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030554A (zh) * | 2010-11-02 | 2011-04-27 | 西安超码科技有限公司 | 一种用天然气混合气cvi致密炭/炭复合材料的方法 |
| CN102060555A (zh) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | 一种高强度炭/炭热压模具的制造方法 |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3927186A (en) * | 1973-02-28 | 1975-12-16 | Chemotronics International Inc | Method for the preparation of carbon structures |
| GB1485528A (en) | 1975-03-24 | 1977-09-14 | Chemotronics International Inc | Method for the preparation of carbon structures |
| GB1485529A (en) | 1975-03-24 | 1977-09-14 | Chemotronics International Inc | Carbon structures |
| JP3151580B2 (ja) | 1992-12-04 | 2001-04-03 | 日石三菱株式会社 | 炭素材料の製造法 |
| US6077464A (en) | 1996-12-19 | 2000-06-20 | Alliedsignal Inc. | Process of making carbon-carbon composite material made from densified carbon foam |
| US6537470B1 (en) | 2000-09-01 | 2003-03-25 | Honeywell International Inc. | Rapid densification of porous bodies (preforms) with high viscosity resins or pitches using a resin transfer molding process |
| US7207424B2 (en) | 2002-12-03 | 2007-04-24 | Ucar Carbon Company Inc. | Manufacture of carbon/carbon composites by hot pressing |
| US6939490B2 (en) | 2002-12-11 | 2005-09-06 | Honeywell International Inc. | Process for unidirectional infiltration of preform with molten resin or pitch |
| GB0401645D0 (en) | 2004-01-26 | 2004-02-25 | Cytec Tech Corp | Stabilizable preform precursors and stabilized preforms for composite materials and processes for stabilizing and debulking preforms |
| FR2879498B1 (fr) | 2004-12-16 | 2009-01-30 | Snecma Propulsion Solide Sa | Densification de structures fibreuses par rtm pour la realisation de pieces en materiau composite |
| US20060177663A1 (en) * | 2005-02-08 | 2006-08-10 | Honeywell International Inc. | Carbon-carbon composite article manufactured with needled fibers |
| FR2926118B1 (fr) | 2008-01-04 | 2010-01-29 | Snecma | Bride en composite avec partie d'usinage. |
| FR2933634B1 (fr) | 2008-07-10 | 2010-08-27 | Snecma | Aube redresseur de soufflante en composite 3d |
| US8801981B2 (en) * | 2008-11-25 | 2014-08-12 | Honeywell International Inc. | Preventing carbon AO migration by limiting surface porosity |
| US20110124253A1 (en) * | 2009-11-23 | 2011-05-26 | Applied Nanostructured Solutions, Llc | Cnt-infused fibers in carbon-carbon composites |
| US9127732B2 (en) | 2011-05-27 | 2015-09-08 | Honeywell International Inc. | Rigidization of porous preform prior to densification |
-
2011
- 2011-05-27 US US13/117,711 patent/US9127732B2/en not_active Expired - Fee Related
-
2012
- 2012-05-14 EP EP20120167950 patent/EP2527129A1/fr not_active Withdrawn
- 2012-05-25 CN CN201210165477.6A patent/CN102795872B/zh not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030554A (zh) * | 2010-11-02 | 2011-04-27 | 西安超码科技有限公司 | 一种用天然气混合气cvi致密炭/炭复合材料的方法 |
| CN102060555A (zh) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | 一种高强度炭/炭热压模具的制造方法 |
Non-Patent Citations (1)
| Title |
|---|
| 医用碳/碳复合材料的制备及骨组织相容性研究;曹宁 等;《山东大学学报（工学报）》;20070228;第37卷(第1期);第1~5页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102795872A (zh) | 2012-11-28 |
| US9127732B2 (en) | 2015-09-08 |
| EP2527129A1 (fr) | 2012-11-28 |
| US20120302117A1 (en) | 2012-11-29 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160921 Termination date: 20190525 |
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| CF01 | Termination of patent right due to non-payment of annual fee |